Phosphorus oxychloride → HCID 178506089, Verbindung

HRID 413240

Reaktionsgleichung

Reaktionsgleichung von HRID 413240
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:12]=[CH:11][C:6]2[NH:7][C:8](=O)[NH:9][C:5]=2[CH:4]=1.O=P(Cl)(Cl)[Cl:17]>>[Cl:17][C:8]1[NH:7][C:6]2[CH:11]=[CH:12][C:3]([C:2]([F:14])([F:13])[F:1])=[CH:4][C:5]=2[N:9]=1

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 118201505-Trifluoromethyl-1,3-dihydro-benzimidazol-2-one

Produkt 1

HCID 178506089HCID 178506089, Verbindung

Versuchsvorschrift

Reflux 5-trifluoromethyl-1,3-dihydro-benzimidazol-2-one (17 g; Meanwell et al. (1995) J. Org. Chem. 60(6):1565-1582) for 14 hours in POCl3 (200 mL). Evaporate the solvent in vacuo, then carefully neutralize with saturated NaHCO3, and extract with EtOAc. Dry over Na2SO4, concentrate under vacuum, and purify by flash chromatography (1 :1 hexanes/EtOAc) to obtain 2-chloro-5-trifluoromethyl-1H-benzimidazole.

Aufarbeitung

  1. customEvaporate the solvent in vacuo
  2. extractionextract with EtOAc
  3. dry with materialDry over Na2SO4
  4. concentrationconcentrate under vacuum
  5. custompurify by flash chromatography (1 :1 hexanes/EtOAc)

Quellen und Nachweise

ORD-Eintrag
ord-fbeaed5d9688447db1d8c343a4d15b84
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06566367B2

Verknüpfte Notizen

Wird geladen…